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Preparation method for 2-amino-4, 6-dimethoxy pyrimidine

A technology of dimethoxypyrimidine and amino, which is applied in the field of preparation of chemical intermediates, can solve the problems of unavailable raw materials of chlorobenzene, harm to people and the environment, and high price, and achieve the reduction of recrystallization links, easy availability of raw materials, high high effect

Inactive Publication Date: 2012-06-13
HUBEI ZHICHENG CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0027] U.S. Patent No. 5,070,201 discloses that 2-amino-4,6-dimethoxypyrimidine is prepared by reacting propanediimine dihydrochloride, monosodium cyanamide, and disodium cyanamide as raw materials in solvent chlorobenzene. Although the operation is simple and the yield is high, the raw materials of monosodium cyanamide, disodium cyanamide, and chlorobenzene are not easy to obtain, expensive, highly toxic, and seriously harmful to humans and the environment

Method used

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  • Preparation method for 2-amino-4, 6-dimethoxy pyrimidine

Examples

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Embodiment 1

[0056] 1. Addition reaction (preparation of 1,3-dimethoxypropanediimine dihydrochloride)

[0057] In a 3000L glass-lined kettle, add metered 1800L methyl acetate through the head tank, start stirring, turn on frozen brine, and cool down to below 0°C; open the vent valve of hydrogen chloride that has been dried, and introduce hydrogen chloride into the kettle, temperature control Below 10°C; when the pressure in the kettle rises to 0.03MPa, the temperature drops, the absorption of hydrogen chloride slows down, and the hydrogen chloride reaches saturation in 3 hours, and then the prepared malononitrile-methanol solution (200kg malononitrile and 270L Methanol, nitrogen gas is filled in the head tank, the pressure in the head tank is higher than the pressure in the kettle), the temperature is 5-10°C, after the dropwise addition (about 5 hours), it is reacted at 15-20°C for 3 hours, and the sampling is controlled in the center; the control is qualified Afterwards, use nitrogen gas ...

Embodiment 2

[0065] 1. Addition reaction (preparation of 1,3-dimethoxypropanediimine dihydrochloride)

[0066] In a 3000L glass-lined kettle, add metered 1800L methyl formate through the head tank, start stirring, turn on frozen brine, and cool down to below 0°C; open the vent valve of hydrogen chloride that has been dried, and introduce hydrogen chloride into the kettle, temperature control Below 10°C; when the pressure in the kettle rises to 0.03MPa, the temperature drops, the absorption of hydrogen chloride slows down, and the hydrogen chloride reaches saturation in 4 hours, and then the prepared malononitrile-methanol solution (200kg malononitrile and 270L Methanol, filled with nitrogen in the head tank, the pressure in the head tank is higher than the pressure in the kettle), the temperature is 5°C, the dropwise addition is completed and reacted at 15°C for 3 hours, and the sampling is controlled in the center; after the control is qualified, press filter, vacuum -0.08MPa and Dry at a...

Embodiment 3

[0074] 1. Addition reaction (preparation of 1,3-dimethoxypropanediimine dihydrochloride)

[0075] In a 3000L glass-lined kettle, add metered 2200L methyl acetate mother liquor (solvent applied separately) through the head tank, start stirring, turn on frozen brine, and cool down to below 0°C; open the dried hydrogen chloride ventilation valve, and vent Add hydrogen chloride, and the temperature is controlled below 10°C; when the pressure in the kettle rises to 0.03MPa, the temperature decreases, the absorption of hydrogen chloride slows down, and the hydrogen chloride reaches saturation in 1.5 hours, then dropwise add the prepared malononitrile-methanol solution (200kg Malononitrile and 250L methanol, nitrogen is filled in the head tank, the pressure in the head tank is higher than the pressure in the kettle), the temperature is 10°C, the dropwise addition is completed and reacted at 15°C for 3 hours, and the sampling is controlled in the middle; after the middle control is qua...

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Abstract

The invention discloses a preparation method for 2-amino-4, 6-dimethoxy pyrimidine, which includes the following steps: 1, malononitrile and methanol are used as raw materials and perform addition reaction in organic solvent to obtain 1, 3-dimethoxy malononitrile imine dihydrochloride; 2, the 1, 3-dimethoxy malononitrile imine dihydrochloride is added in alkali solution, and cyanamide and disodium hydrogen phosphate are added in the alkali solution to perform cyanamide reaction so as to obtain 3-amino-3-methoxyl-N-cyan-2-propionamidine; and 3, the 3-amino-3-methoxyl-N-cyan-2-propionamidine is added in toluene solution, stabilizing agent is added in the toluene solution to perform ring closing reaction so as to obtain 2-amino-4, 6-dimethoxy pyrimidine. The preparation method is safe, environment-friendly, economical, high in yield and purity and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a chemical intermediate, in particular to a preparation method of 2-amino-4,6-dimethoxypyrimidine. Background technique [0002] Sulfonylurea herbicides are broad-spectrum and high-efficiency herbicides for rice, corn, and soybean fields. They have the characteristics of high activity, low dosage and low toxicity. They are recognized as high-efficiency, environmentally friendly green pesticides in the world. At present, there are more than 30 commercialized products. In recent years, as some herbicides with environmental problems have faded out of the market, sulfonylurea herbicides have developed rapidly. The current sales market is only second to amino acid herbicides such as glyphosate. In 2010, the global sales were nearly 2.5 billion US dollars. Use very large amounts. China is a big rice producing country. Due to the perennial use of herbicides such as butachlor and quinclorac, the weed community...

Claims

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Application Information

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IPC IPC(8): C07D239/52
Inventor 张闰扬
Owner HUBEI ZHICHENG CHEM TECH
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